Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805033416/bt6762sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805033416/bt6762Isup2.hkl |
CCDC reference: 274082
Data collection: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis RED (Oxford Diffraction, 2003); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: enCIFer (Allen et al., 2004).
[Mn3(C2Cl3O2)6O(C2H4O2)3] | Z = 2 |
Mr = 1335.20 | F(000) = 1306 |
Triclinic, P1 | Dx = 2.047 Mg m−3 Dm = 1.943 Mg m−3 Dm measured by flotation |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.121 (3) Å | Cell parameters from 18242 reflections |
b = 10.424 (3) Å | θ = 0–27.6° |
c = 22.891 (5) Å | µ = 2.04 mm−1 |
α = 88.01 (3)° | T = 100 K |
β = 79.45 (3)° | Parallelepiped, dark brown |
γ = 65.94 (3)° | 0.2 × 0.2 × 0.05 mm |
V = 2165.8 (12) Å3 |
Kuma KM-4 CCD κ-geometry diffractometer | 9906 independent reflections |
Radiation source: long fine focus sealed tube | 8642 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
ω–2θ scans | θmax = 27.6°, θmin = 3.1° |
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2003) | h = −13→12 |
Tmin = 0.691, Tmax = 0.899 | k = −13→13 |
30649 measured reflections | l = −29→29 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.054 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.097 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.16 | w = 1/[σ2(Fo2) + (0.0043P)2 + 12.065P] where P = (Fo2 + 2Fc2)/3 |
9906 reflections | (Δ/σ)max = 0.001 |
532 parameters | Δρmax = 0.64 e Å−3 |
0 restraints | Δρmin = −0.55 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Mn1 | 0.69672 (6) | 0.17138 (6) | 0.25769 (3) | 0.00843 (12) | |
Mn2 | 0.97456 (6) | 0.21472 (6) | 0.28833 (3) | 0.00837 (12) | |
Mn3 | 0.73499 (6) | 0.47241 (6) | 0.21352 (3) | 0.00915 (12) | |
Cl11 | 1.26888 (12) | −0.27124 (12) | 0.18781 (5) | 0.0233 (2) | |
Cl12 | 1.06140 (15) | −0.12506 (14) | 0.11193 (5) | 0.0327 (3) | |
Cl13 | 0.99502 (13) | −0.30211 (12) | 0.20187 (6) | 0.0272 (3) | |
Cl21 | 0.58104 (12) | 0.10169 (12) | 0.47254 (5) | 0.0196 (2) | |
Cl22 | 0.75838 (13) | 0.25078 (13) | 0.48664 (5) | 0.0250 (2) | |
Cl23 | 0.89466 (12) | −0.05113 (13) | 0.46058 (5) | 0.0236 (2) | |
Cl31 | 1.19043 (12) | 0.42299 (13) | 0.07144 (5) | 0.0274 (3) | |
Cl32 | 1.27315 (13) | 0.13067 (12) | 0.09810 (5) | 0.0261 (3) | |
Cl33 | 1.35384 (11) | 0.30987 (13) | 0.16485 (5) | 0.0235 (2) | |
Cl41 | 0.72961 (17) | 0.81369 (12) | 0.35604 (6) | 0.0337 (3) | |
Cl42 | 0.85534 (14) | 0.60474 (12) | 0.43831 (5) | 0.0262 (3) | |
Cl43 | 0.57796 (14) | 0.64312 (18) | 0.40811 (7) | 0.0425 (4) | |
Cl51 | 0.71097 (14) | 0.08130 (12) | 0.04108 (5) | 0.0240 (2) | |
Cl52 | 0.93105 (12) | 0.19383 (14) | 0.03650 (5) | 0.0255 (2) | |
Cl53 | 0.63743 (13) | 0.37306 (12) | 0.01974 (5) | 0.0248 (2) | |
Cl61 | 0.24622 (12) | 0.71116 (11) | 0.34557 (5) | 0.0236 (2) | |
Cl62 | 0.35107 (13) | 0.45018 (13) | 0.40540 (5) | 0.0253 (2) | |
Cl63 | 0.18499 (12) | 0.48050 (13) | 0.31160 (5) | 0.0240 (2) | |
O1 | 0.8088 (3) | 0.2719 (3) | 0.25548 (12) | 0.0100 (5) | |
O11 | 0.8624 (3) | −0.0108 (3) | 0.23794 (13) | 0.0128 (6) | |
O12 | 1.0735 (3) | 0.0082 (3) | 0.24231 (13) | 0.0153 (6) | |
O21 | 0.6839 (3) | 0.1371 (3) | 0.35147 (12) | 0.0139 (6) | |
O22 | 0.8968 (3) | 0.1461 (3) | 0.36144 (13) | 0.0156 (6) | |
O31 | 1.0926 (3) | 0.2720 (3) | 0.22234 (12) | 0.0138 (6) | |
O32 | 0.9552 (3) | 0.4109 (3) | 0.15956 (13) | 0.0136 (6) | |
O41 | 0.8969 (3) | 0.4103 (3) | 0.34092 (13) | 0.0132 (6) | |
O42 | 0.7881 (3) | 0.5745 (3) | 0.27944 (13) | 0.0143 (6) | |
O51 | 0.6841 (3) | 0.3873 (3) | 0.14049 (13) | 0.0150 (6) | |
O52 | 0.7061 (3) | 0.1692 (3) | 0.16087 (12) | 0.0131 (6) | |
O61 | 0.5209 (3) | 0.5430 (3) | 0.26928 (13) | 0.0141 (6) | |
O62 | 0.5069 (3) | 0.3338 (3) | 0.27940 (13) | 0.0134 (6) | |
O71 | 0.5714 (3) | 0.0653 (3) | 0.26212 (12) | 0.0126 (6) | |
O72 | 0.6205 (4) | −0.0377 (3) | 0.17107 (14) | 0.0205 (7) | |
H72 | 0.656 (7) | 0.016 (6) | 0.165 (3) | 0.031* | |
O81 | 1.1535 (3) | 0.1542 (3) | 0.32471 (13) | 0.0128 (6) | |
O82 | 1.0811 (4) | 0.2750 (3) | 0.41261 (14) | 0.0187 (7) | |
H82 | 1.009 (7) | 0.316 (6) | 0.404 (3) | 0.028* | |
O91 | 0.6679 (3) | 0.6515 (3) | 0.15823 (13) | 0.0159 (6) | |
O92 | 0.8317 (4) | 0.5976 (4) | 0.07311 (15) | 0.0282 (8) | |
H92 | 0.883 (7) | 0.562 (7) | 0.093 (3) | 0.042* | |
C11 | 1.0013 (4) | −0.0503 (4) | 0.22658 (17) | 0.0115 (8) | |
C12 | 1.0821 (5) | −0.1857 (5) | 0.18463 (19) | 0.0158 (8) | |
C21 | 0.7769 (4) | 0.1339 (4) | 0.37980 (18) | 0.0121 (8) | |
C22 | 0.7521 (4) | 0.1097 (4) | 0.44757 (18) | 0.0133 (8) | |
C31 | 1.0726 (4) | 0.3337 (4) | 0.17443 (17) | 0.0100 (7) | |
C32 | 1.2175 (4) | 0.3034 (4) | 0.12863 (18) | 0.0143 (8) | |
C41 | 0.8214 (4) | 0.5336 (4) | 0.32749 (18) | 0.0122 (8) | |
C42 | 0.7527 (5) | 0.6457 (5) | 0.3807 (2) | 0.0183 (9) | |
C51 | 0.7039 (4) | 0.2667 (4) | 0.12671 (18) | 0.0111 (8) | |
C52 | 0.7424 (5) | 0.2294 (4) | 0.05845 (18) | 0.0143 (8) | |
C61 | 0.4629 (4) | 0.4639 (4) | 0.29003 (18) | 0.0112 (8) | |
C62 | 0.3157 (4) | 0.5266 (4) | 0.33616 (19) | 0.0152 (8) | |
C71 | 0.5578 (4) | −0.0164 (4) | 0.22697 (19) | 0.0130 (8) | |
C72 | 0.4644 (5) | −0.0938 (5) | 0.2479 (2) | 0.0187 (9) | |
H72A | 0.4974 | −0.1479 | 0.2822 | 0.028* | |
H72B | 0.4725 | −0.1580 | 0.2158 | 0.028* | |
H72C | 0.3616 | −0.0267 | 0.2594 | 0.028* | |
C81 | 1.1753 (5) | 0.1769 (4) | 0.37398 (18) | 0.0138 (8) | |
C82 | 1.3175 (5) | 0.0934 (5) | 0.3935 (2) | 0.0230 (10) | |
H82A | 1.3414 | −0.0071 | 0.3886 | 0.035* | |
H82B | 1.3089 | 0.1173 | 0.4355 | 0.035* | |
H82C | 1.3957 | 0.1151 | 0.3694 | 0.035* | |
C91 | 0.6995 (5) | 0.6677 (4) | 0.10538 (19) | 0.0149 (8) | |
C92 | 0.5922 (5) | 0.7670 (5) | 0.0710 (2) | 0.0219 (10) | |
H92A | 0.5179 | 0.7317 | 0.0671 | 0.033* | |
H92B | 0.6439 | 0.7750 | 0.0314 | 0.033* | |
H92C | 0.5439 | 0.8596 | 0.0918 | 0.033* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0075 (3) | 0.0084 (3) | 0.0097 (3) | −0.0037 (2) | −0.0013 (2) | 0.0004 (2) |
Mn2 | 0.0071 (3) | 0.0097 (3) | 0.0088 (3) | −0.0038 (2) | −0.0018 (2) | 0.0006 (2) |
Mn3 | 0.0086 (3) | 0.0087 (3) | 0.0094 (3) | −0.0032 (2) | −0.0007 (2) | 0.0002 (2) |
Cl11 | 0.0140 (5) | 0.0188 (5) | 0.0332 (6) | −0.0025 (4) | −0.0034 (4) | −0.0057 (5) |
Cl12 | 0.0370 (7) | 0.0350 (7) | 0.0140 (5) | −0.0026 (6) | −0.0041 (5) | −0.0018 (5) |
Cl13 | 0.0217 (5) | 0.0144 (5) | 0.0459 (7) | −0.0086 (4) | −0.0026 (5) | −0.0054 (5) |
Cl21 | 0.0179 (5) | 0.0316 (6) | 0.0140 (5) | −0.0157 (5) | −0.0012 (4) | 0.0034 (4) |
Cl22 | 0.0293 (6) | 0.0326 (6) | 0.0187 (5) | −0.0202 (5) | 0.0024 (4) | −0.0100 (5) |
Cl23 | 0.0223 (5) | 0.0267 (6) | 0.0211 (5) | −0.0082 (5) | −0.0086 (4) | 0.0096 (5) |
Cl31 | 0.0179 (5) | 0.0344 (7) | 0.0203 (5) | −0.0049 (5) | 0.0036 (4) | 0.0125 (5) |
Cl32 | 0.0239 (6) | 0.0215 (6) | 0.0261 (6) | −0.0053 (5) | 0.0042 (5) | −0.0102 (5) |
Cl33 | 0.0124 (5) | 0.0368 (6) | 0.0239 (6) | −0.0132 (5) | −0.0020 (4) | 0.0000 (5) |
Cl41 | 0.0579 (8) | 0.0129 (5) | 0.0327 (7) | −0.0101 (5) | −0.0242 (6) | −0.0007 (5) |
Cl42 | 0.0384 (7) | 0.0201 (5) | 0.0184 (5) | −0.0067 (5) | −0.0131 (5) | −0.0022 (4) |
Cl43 | 0.0227 (6) | 0.0616 (10) | 0.0386 (8) | −0.0182 (6) | 0.0137 (5) | −0.0277 (7) |
Cl51 | 0.0411 (7) | 0.0220 (6) | 0.0150 (5) | −0.0186 (5) | −0.0051 (5) | −0.0030 (4) |
Cl52 | 0.0169 (5) | 0.0377 (7) | 0.0184 (5) | −0.0096 (5) | 0.0022 (4) | −0.0033 (5) |
Cl53 | 0.0333 (6) | 0.0219 (6) | 0.0176 (5) | −0.0062 (5) | −0.0140 (5) | 0.0063 (4) |
Cl61 | 0.0196 (5) | 0.0155 (5) | 0.0285 (6) | −0.0031 (4) | 0.0046 (4) | −0.0054 (4) |
Cl62 | 0.0312 (6) | 0.0296 (6) | 0.0140 (5) | −0.0130 (5) | −0.0003 (4) | 0.0025 (4) |
Cl63 | 0.0124 (5) | 0.0297 (6) | 0.0310 (6) | −0.0106 (4) | −0.0013 (4) | −0.0023 (5) |
O1 | 0.0118 (13) | 0.0094 (13) | 0.0111 (13) | −0.0067 (11) | −0.0024 (10) | 0.0015 (11) |
O11 | 0.0122 (13) | 0.0107 (14) | 0.0147 (14) | −0.0047 (11) | −0.0005 (11) | −0.0019 (11) |
O12 | 0.0114 (14) | 0.0135 (14) | 0.0202 (15) | −0.0039 (12) | −0.0035 (12) | −0.0026 (12) |
O21 | 0.0158 (14) | 0.0196 (15) | 0.0103 (13) | −0.0110 (12) | −0.0031 (11) | 0.0010 (12) |
O22 | 0.0139 (14) | 0.0226 (16) | 0.0118 (14) | −0.0092 (13) | −0.0025 (11) | 0.0046 (12) |
O31 | 0.0095 (13) | 0.0215 (15) | 0.0099 (14) | −0.0066 (12) | −0.0012 (11) | 0.0048 (12) |
O32 | 0.0119 (14) | 0.0146 (14) | 0.0126 (14) | −0.0042 (12) | −0.0018 (11) | 0.0026 (11) |
O41 | 0.0131 (14) | 0.0117 (14) | 0.0138 (14) | −0.0031 (11) | −0.0044 (11) | −0.0018 (11) |
O42 | 0.0175 (14) | 0.0131 (14) | 0.0153 (15) | −0.0086 (12) | −0.0050 (12) | −0.0001 (12) |
O51 | 0.0189 (15) | 0.0137 (14) | 0.0142 (14) | −0.0075 (12) | −0.0048 (12) | −0.0014 (12) |
O52 | 0.0187 (14) | 0.0118 (14) | 0.0091 (13) | −0.0064 (12) | −0.0027 (11) | 0.0002 (11) |
O61 | 0.0111 (13) | 0.0113 (14) | 0.0166 (15) | −0.0028 (11) | 0.0008 (11) | 0.0003 (12) |
O62 | 0.0087 (13) | 0.0107 (14) | 0.0194 (15) | −0.0031 (11) | −0.0004 (11) | −0.0021 (12) |
O71 | 0.0111 (13) | 0.0153 (14) | 0.0126 (14) | −0.0070 (11) | −0.0009 (11) | −0.0020 (11) |
O72 | 0.0313 (18) | 0.0199 (17) | 0.0169 (16) | −0.0177 (15) | −0.0030 (13) | 0.0010 (13) |
O81 | 0.0118 (13) | 0.0138 (14) | 0.0132 (14) | −0.0056 (11) | −0.0025 (11) | 0.0020 (11) |
O82 | 0.0154 (15) | 0.0207 (17) | 0.0174 (16) | −0.0033 (13) | −0.0064 (12) | 0.0001 (13) |
O91 | 0.0214 (15) | 0.0092 (14) | 0.0158 (15) | −0.0049 (12) | −0.0033 (12) | 0.0000 (12) |
O92 | 0.0174 (17) | 0.039 (2) | 0.0185 (17) | −0.0023 (16) | −0.0035 (13) | 0.0116 (15) |
C11 | 0.0121 (18) | 0.0114 (19) | 0.0097 (18) | −0.0032 (15) | −0.0027 (15) | 0.0031 (15) |
C12 | 0.0115 (19) | 0.017 (2) | 0.015 (2) | −0.0025 (16) | −0.0016 (15) | 0.0019 (17) |
C21 | 0.0126 (18) | 0.0071 (18) | 0.0134 (19) | −0.0016 (15) | −0.0002 (15) | 0.0010 (15) |
C22 | 0.0151 (19) | 0.017 (2) | 0.0105 (19) | −0.0093 (17) | −0.0023 (15) | 0.0008 (16) |
C31 | 0.0093 (17) | 0.0086 (18) | 0.0105 (18) | −0.0028 (15) | 0.0002 (14) | −0.0017 (15) |
C32 | 0.0111 (18) | 0.017 (2) | 0.0128 (19) | −0.0046 (16) | −0.0001 (15) | 0.0016 (16) |
C41 | 0.0104 (18) | 0.0130 (19) | 0.015 (2) | −0.0071 (16) | −0.0016 (15) | −0.0015 (16) |
C42 | 0.021 (2) | 0.015 (2) | 0.018 (2) | −0.0054 (17) | −0.0049 (17) | −0.0031 (17) |
C51 | 0.0061 (17) | 0.015 (2) | 0.0120 (19) | −0.0039 (15) | −0.0024 (14) | 0.0005 (15) |
C52 | 0.018 (2) | 0.014 (2) | 0.0117 (19) | −0.0078 (17) | −0.0007 (16) | 0.0015 (16) |
C61 | 0.0057 (17) | 0.0147 (19) | 0.0121 (19) | −0.0025 (15) | −0.0027 (14) | 0.0004 (15) |
C62 | 0.0128 (19) | 0.016 (2) | 0.016 (2) | −0.0064 (16) | 0.0012 (16) | 0.0004 (17) |
C71 | 0.0125 (19) | 0.0088 (18) | 0.017 (2) | −0.0033 (15) | −0.0037 (15) | −0.0012 (16) |
C72 | 0.017 (2) | 0.018 (2) | 0.024 (2) | −0.0131 (18) | 0.0038 (17) | −0.0057 (18) |
C81 | 0.0151 (19) | 0.016 (2) | 0.0137 (19) | −0.0106 (17) | −0.0024 (15) | 0.0039 (16) |
C82 | 0.016 (2) | 0.030 (3) | 0.022 (2) | −0.0064 (19) | −0.0080 (18) | 0.008 (2) |
C91 | 0.018 (2) | 0.014 (2) | 0.017 (2) | −0.0087 (17) | −0.0070 (16) | 0.0001 (16) |
C92 | 0.025 (2) | 0.024 (2) | 0.013 (2) | −0.0040 (19) | −0.0064 (18) | 0.0028 (18) |
Mn1—O1 | 1.826 (3) | O11—C11 | 1.271 (5) |
Mn1—O11 | 1.952 (3) | O12—C11 | 1.228 (5) |
Mn1—O62 | 1.965 (3) | O21—C21 | 1.227 (5) |
Mn1—O71 | 1.983 (3) | O22—C21 | 1.265 (5) |
Mn1—O21 | 2.153 (3) | O31—C31 | 1.258 (5) |
Mn1—O52 | 2.201 (3) | O32—C31 | 1.235 (5) |
Mn2—O1 | 1.830 (3) | O41—C41 | 1.260 (5) |
Mn2—O22 | 1.956 (3) | O42—C41 | 1.221 (5) |
Mn2—O31 | 1.981 (3) | O51—C51 | 1.233 (5) |
Mn2—O81 | 1.989 (3) | O52—C51 | 1.256 (5) |
Mn2—O41 | 2.178 (3) | O61—C61 | 1.232 (5) |
Mn2—O12 | 2.182 (3) | O62—C61 | 1.260 (5) |
Mn3—O42 | 2.139 (3) | O71—C71 | 1.255 (5) |
Mn3—O61 | 2.149 (3) | O72—C71 | 1.303 (5) |
Mn3—O51 | 2.153 (3) | O72—H72 | 0.78 (6) |
Mn3—O91 | 2.160 (3) | O81—C81 | 1.237 (5) |
Mn3—O1 | 2.167 (3) | O82—C81 | 1.302 (5) |
Mn3—O32 | 2.188 (3) | O82—H82 | 0.75 (6) |
Mn1—Mn2 | 3.2223 (12) | O91—C91 | 1.218 (5) |
Mn1—Mn3 | 3.4126 (13) | O92—C91 | 1.322 (5) |
Mn2—Mn3 | 3.4521 (16) | O92—H92 | 0.72 (7) |
Cl11—C12 | 1.745 (4) | C11—C12 | 1.565 (6) |
Cl12—C12 | 1.778 (4) | C21—C22 | 1.554 (6) |
Cl13—C12 | 1.766 (5) | C31—C32 | 1.560 (5) |
Cl21—C22 | 1.755 (4) | C41—C42 | 1.569 (6) |
Cl22—C22 | 1.777 (4) | C51—C52 | 1.562 (6) |
Cl23—C22 | 1.770 (4) | C61—C62 | 1.562 (5) |
Cl31—C32 | 1.756 (4) | C71—C72 | 1.484 (6) |
Cl32—C32 | 1.779 (4) | C72—H72A | 0.9800 |
Cl33—C32 | 1.759 (4) | C72—H72B | 0.9800 |
Cl41—C42 | 1.757 (5) | C72—H72C | 0.9800 |
Cl42—C42 | 1.760 (5) | C81—C82 | 1.489 (6) |
Cl43—C42 | 1.776 (5) | C82—H82A | 0.9800 |
Cl51—C52 | 1.769 (4) | C82—H82B | 0.9800 |
Cl52—C52 | 1.766 (4) | C82—H82C | 0.9800 |
Cl53—C52 | 1.764 (4) | C91—C92 | 1.487 (6) |
Cl61—C62 | 1.764 (4) | C92—H92A | 0.9800 |
Cl62—C62 | 1.778 (5) | C92—H92B | 0.9800 |
Cl63—C62 | 1.762 (4) | C92—H92C | 0.9800 |
O1—Mn1—O11 | 95.63 (12) | O11—C11—C12 | 112.9 (3) |
O1—Mn1—O62 | 95.31 (12) | C11—C12—Cl11 | 112.7 (3) |
O11—Mn1—O62 | 169.02 (12) | C11—C12—Cl13 | 110.1 (3) |
O1—Mn1—O71 | 178.40 (12) | Cl11—C12—Cl13 | 110.1 (2) |
O11—Mn1—O71 | 85.54 (12) | C11—C12—Cl12 | 104.9 (3) |
O62—Mn1—O71 | 83.50 (12) | Cl11—C12—Cl12 | 109.7 (2) |
O1—Mn1—O21 | 94.76 (12) | Cl13—C12—Cl12 | 109.2 (2) |
O11—Mn1—O21 | 91.62 (12) | O21—C21—O22 | 128.9 (4) |
O62—Mn1—O21 | 86.55 (13) | O21—C21—C22 | 118.6 (3) |
O71—Mn1—O21 | 84.11 (12) | O22—C21—C22 | 112.5 (4) |
O1—Mn1—O52 | 94.51 (12) | C21—C22—Cl21 | 111.6 (3) |
O11—Mn1—O52 | 82.32 (12) | C21—C22—Cl23 | 108.0 (3) |
O62—Mn1—O52 | 97.73 (12) | Cl21—C22—Cl23 | 109.4 (2) |
O71—Mn1—O52 | 86.71 (12) | C21—C22—Cl22 | 108.8 (3) |
O21—Mn1—O52 | 169.38 (11) | Cl21—C22—Cl22 | 108.9 (2) |
O1—Mn1—Mn2 | 28.23 (9) | Cl23—C22—Cl22 | 110.1 (2) |
O11—Mn1—Mn2 | 75.24 (9) | O32—C31—O31 | 128.5 (4) |
O62—Mn1—Mn2 | 114.68 (9) | O32—C31—C32 | 117.7 (3) |
O71—Mn1—Mn2 | 151.83 (9) | O31—C31—C32 | 113.8 (3) |
O21—Mn1—Mn2 | 76.18 (8) | C31—C32—Cl31 | 112.1 (3) |
O52—Mn1—Mn2 | 110.38 (8) | C31—C32—Cl33 | 110.1 (3) |
O1—Mn2—O22 | 96.73 (12) | Cl31—C32—Cl33 | 109.4 (2) |
O1—Mn2—O31 | 95.98 (12) | C31—C32—Cl32 | 105.8 (3) |
O22—Mn2—O31 | 167.29 (12) | Cl31—C32—Cl32 | 109.5 (2) |
O1—Mn2—O81 | 179.38 (13) | Cl33—C32—Cl32 | 109.9 (2) |
O22—Mn2—O81 | 83.02 (12) | O42—C41—O41 | 128.3 (4) |
O31—Mn2—O81 | 84.27 (12) | O42—C41—C42 | 116.4 (4) |
O1—Mn2—O41 | 93.53 (12) | O41—C41—C42 | 115.2 (4) |
O22—Mn2—O41 | 84.29 (12) | C41—C42—Cl42 | 113.5 (3) |
O31—Mn2—O41 | 94.51 (12) | C41—C42—Cl41 | 110.9 (3) |
O81—Mn2—O41 | 85.88 (12) | Cl42—C42—Cl41 | 109.4 (2) |
O1—Mn2—O12 | 93.38 (12) | C41—C42—Cl43 | 104.1 (3) |
O22—Mn2—O12 | 93.38 (13) | Cl42—C42—Cl43 | 109.1 (3) |
O31—Mn2—O12 | 86.29 (12) | Cl41—C42—Cl43 | 109.7 (2) |
O81—Mn2—O12 | 87.20 (12) | O51—C51—O52 | 127.6 (4) |
O41—Mn2—O12 | 172.92 (11) | O51—C51—C52 | 115.3 (4) |
O1—Mn2—Mn1 | 28.15 (9) | O52—C51—C52 | 116.9 (3) |
O22—Mn2—Mn1 | 75.69 (9) | C51—C52—Cl53 | 110.5 (3) |
O31—Mn2—Mn1 | 116.43 (9) | C51—C52—Cl52 | 105.9 (3) |
O81—Mn2—Mn1 | 152.03 (9) | Cl53—C52—Cl52 | 109.5 (2) |
O41—Mn2—Mn1 | 109.44 (8) | C51—C52—Cl51 | 112.4 (3) |
O12—Mn2—Mn1 | 76.32 (8) | Cl53—C52—Cl51 | 108.5 (2) |
O42—Mn3—O61 | 85.28 (12) | Cl52—C52—Cl51 | 110.0 (2) |
O42—Mn3—O51 | 173.55 (11) | O61—C61—O62 | 128.5 (4) |
O61—Mn3—O51 | 97.21 (12) | O61—C61—C62 | 118.5 (4) |
O42—Mn3—O91 | 95.39 (11) | O62—C61—C62 | 113.0 (3) |
O61—Mn3—O91 | 92.84 (12) | C61—C62—Cl61 | 112.6 (3) |
O51—Mn3—O91 | 78.58 (12) | C61—C62—Cl63 | 108.4 (3) |
O42—Mn3—O1 | 93.47 (11) | Cl61—C62—Cl63 | 109.5 (2) |
O61—Mn3—O1 | 91.65 (11) | C61—C62—Cl62 | 107.7 (3) |
O51—Mn3—O1 | 92.41 (11) | Cl61—C62—Cl62 | 109.0 (2) |
O91—Mn3—O1 | 170.37 (11) | Cl63—C62—Cl62 | 109.7 (2) |
O42—Mn3—O32 | 91.30 (12) | O71—C71—O72 | 123.6 (4) |
O61—Mn3—O32 | 176.36 (12) | O71—C71—C72 | 120.3 (4) |
O51—Mn3—O32 | 86.06 (12) | O72—C71—C72 | 116.0 (4) |
O91—Mn3—O32 | 86.22 (12) | C71—C72—H72A | 109.5 |
O1—Mn3—O32 | 89.82 (11) | C71—C72—H72B | 109.5 |
Mn1—O1—Mn2 | 123.61 (15) | H72A—C72—H72B | 109.5 |
Mn1—O1—Mn3 | 117.18 (14) | C71—C72—H72C | 109.5 |
Mn2—O1—Mn3 | 119.18 (14) | H72A—C72—H72C | 109.5 |
C11—O11—Mn1 | 133.7 (3) | H72B—C72—H72C | 109.5 |
C11—O12—Mn2 | 123.4 (3) | O81—C81—O82 | 124.6 (4) |
C21—O21—Mn1 | 124.3 (3) | O81—C81—C82 | 121.5 (4) |
C21—O22—Mn2 | 133.2 (3) | O82—C81—C82 | 113.9 (4) |
C31—O31—Mn2 | 137.0 (3) | C81—C82—H82A | 109.5 |
C31—O32—Mn3 | 126.3 (3) | C81—C82—H82B | 109.5 |
C41—O41—Mn2 | 128.6 (3) | H82A—C82—H82B | 109.5 |
C41—O42—Mn3 | 129.4 (3) | C81—C82—H82C | 109.5 |
C51—O51—Mn3 | 132.2 (3) | H82A—C82—H82C | 109.5 |
C51—O52—Mn1 | 127.0 (3) | H82B—C82—H82C | 109.5 |
C61—O61—Mn3 | 123.9 (3) | O91—C91—O92 | 123.2 (4) |
C61—O62—Mn1 | 137.2 (3) | O91—C91—C92 | 123.0 (4) |
C71—O71—Mn1 | 134.7 (3) | O92—C91—C92 | 113.8 (4) |
C71—O72—H72 | 106 (4) | C91—C92—H92A | 109.5 |
C81—O81—Mn2 | 133.7 (3) | C91—C92—H92B | 109.5 |
C81—O82—H82 | 115 (5) | H92A—C92—H92B | 109.5 |
C91—O91—Mn3 | 133.7 (3) | C91—C92—H92C | 109.5 |
C91—O92—H92 | 109 (5) | H92A—C92—H92C | 109.5 |
O12—C11—O11 | 127.8 (4) | H92B—C92—H92C | 109.5 |
O12—C11—C12 | 119.2 (3) | ||
O11—Mn1—Mn2—O1 | 134.8 (2) | O32—Mn3—O42—C41 | −101.3 (3) |
O62—Mn1—Mn2—O1 | −50.2 (2) | O61—Mn3—O51—C51 | −97.7 (4) |
O71—Mn1—Mn2—O1 | −176.6 (3) | O91—Mn3—O51—C51 | 170.9 (4) |
O21—Mn1—Mn2—O1 | −129.7 (2) | O1—Mn3—O51—C51 | −5.7 (4) |
O52—Mn1—Mn2—O1 | 59.0 (2) | O32—Mn3—O51—C51 | 84.0 (4) |
O1—Mn1—Mn2—O22 | 137.1 (2) | O1—Mn1—O52—C51 | −37.1 (3) |
O11—Mn1—Mn2—O22 | −88.03 (13) | O11—Mn1—O52—C51 | −132.2 (3) |
O62—Mn1—Mn2—O22 | 86.98 (14) | O62—Mn1—O52—C51 | 58.9 (3) |
O71—Mn1—Mn2—O22 | −39.5 (2) | O71—Mn1—O52—C51 | 141.9 (3) |
O21—Mn1—Mn2—O22 | 7.42 (12) | O21—Mn1—O52—C51 | 172.2 (5) |
O52—Mn1—Mn2—O22 | −163.83 (12) | Mn2—Mn1—O52—C51 | −61.1 (3) |
O1—Mn1—Mn2—O31 | −47.0 (2) | O42—Mn3—O61—C61 | −122.6 (3) |
O11—Mn1—Mn2—O31 | 87.87 (14) | O51—Mn3—O61—C61 | 63.4 (3) |
O62—Mn1—Mn2—O31 | −97.13 (14) | O91—Mn3—O61—C61 | 142.2 (3) |
O71—Mn1—Mn2—O31 | 136.4 (2) | O1—Mn3—O61—C61 | −29.3 (3) |
O21—Mn1—Mn2—O31 | −176.68 (13) | O1—Mn1—O62—C61 | −0.9 (4) |
O52—Mn1—Mn2—O31 | 12.07 (13) | O11—Mn1—O62—C61 | 174.2 (6) |
O1—Mn1—Mn2—O81 | 178.7 (3) | O71—Mn1—O62—C61 | 178.0 (4) |
O11—Mn1—Mn2—O81 | −46.4 (2) | O21—Mn1—O62—C61 | 93.6 (4) |
O62—Mn1—Mn2—O81 | 128.6 (2) | O52—Mn1—O62—C61 | −96.2 (4) |
O71—Mn1—Mn2—O81 | 2.1 (3) | Mn2—Mn1—O62—C61 | 20.5 (4) |
O21—Mn1—Mn2—O81 | 49.0 (2) | O11—Mn1—O71—C71 | −56.0 (4) |
O52—Mn1—Mn2—O81 | −122.2 (2) | O62—Mn1—O71—C71 | 124.7 (4) |
O1—Mn1—Mn2—O41 | 58.6 (2) | O21—Mn1—O71—C71 | −148.1 (4) |
O11—Mn1—Mn2—O41 | −166.56 (12) | O52—Mn1—O71—C71 | 26.5 (4) |
O62—Mn1—Mn2—O41 | 8.45 (13) | Mn2—Mn1—O71—C71 | −102.6 (4) |
O71—Mn1—Mn2—O41 | −118.0 (2) | O22—Mn2—O81—C81 | −51.1 (4) |
O21—Mn1—Mn2—O41 | −71.11 (12) | O31—Mn2—O81—C81 | 128.6 (4) |
O52—Mn1—Mn2—O41 | 117.64 (12) | O41—Mn2—O81—C81 | 33.7 (4) |
O1—Mn1—Mn2—O12 | −125.7 (2) | O12—Mn2—O81—C81 | −144.8 (4) |
O11—Mn1—Mn2—O12 | 9.14 (12) | Mn1—Mn2—O81—C81 | −91.5 (4) |
O62—Mn1—Mn2—O12 | −175.86 (13) | O42—Mn3—O91—C91 | 129.6 (4) |
O71—Mn1—Mn2—O12 | 57.7 (2) | O61—Mn3—O91—C91 | −144.9 (4) |
O21—Mn1—Mn2—O12 | 104.59 (12) | O51—Mn3—O91—C91 | −48.1 (4) |
O52—Mn1—Mn2—O12 | −66.66 (12) | O32—Mn3—O91—C91 | 38.6 (4) |
O11—Mn1—O1—Mn2 | −43.55 (19) | Mn2—O12—C11—O11 | −6.7 (6) |
O62—Mn1—O1—Mn2 | 135.52 (18) | Mn2—O12—C11—C12 | 169.7 (3) |
O21—Mn1—O1—Mn2 | 48.56 (19) | Mn1—O11—C11—O12 | 24.9 (7) |
O52—Mn1—O1—Mn2 | −126.26 (18) | Mn1—O11—C11—C12 | −151.7 (3) |
O11—Mn1—O1—Mn3 | 138.22 (15) | O12—C11—C12—Cl11 | 22.3 (5) |
O62—Mn1—O1—Mn3 | −42.70 (16) | O11—C11—C12—Cl11 | −160.8 (3) |
O21—Mn1—O1—Mn3 | −129.67 (15) | O12—C11—C12—Cl13 | 145.8 (3) |
O52—Mn1—O1—Mn3 | 55.51 (15) | O11—C11—C12—Cl13 | −37.3 (4) |
Mn2—Mn1—O1—Mn3 | −178.2 (3) | O12—C11—C12—Cl12 | −96.9 (4) |
O22—Mn2—O1—Mn1 | −41.59 (19) | O11—C11—C12—Cl12 | 80.0 (4) |
O31—Mn2—O1—Mn1 | 138.84 (18) | Mn1—O21—C21—O22 | −1.8 (6) |
O41—Mn2—O1—Mn1 | −126.25 (18) | Mn1—O21—C21—C22 | 179.4 (3) |
O12—Mn2—O1—Mn1 | 52.22 (18) | Mn2—O22—C21—O21 | 15.9 (7) |
O22—Mn2—O1—Mn3 | 136.60 (16) | Mn2—O22—C21—C22 | −165.2 (3) |
O31—Mn2—O1—Mn3 | −42.97 (17) | O21—C21—C22—Cl21 | −3.8 (5) |
O41—Mn2—O1—Mn3 | 51.94 (16) | O22—C21—C22—Cl21 | 177.1 (3) |
O12—Mn2—O1—Mn3 | −129.59 (15) | O21—C21—C22—Cl23 | 116.4 (4) |
Mn1—Mn2—O1—Mn3 | 178.2 (3) | O22—C21—C22—Cl23 | −62.6 (4) |
O42—Mn3—O1—Mn1 | 139.22 (15) | O21—C21—C22—Cl22 | −124.0 (3) |
O61—Mn3—O1—Mn1 | 53.85 (16) | O22—C21—C22—Cl22 | 56.9 (4) |
O51—Mn3—O1—Mn1 | −43.44 (16) | Mn3—O32—C31—O31 | 1.3 (6) |
O32—Mn3—O1—Mn1 | −129.49 (16) | Mn3—O32—C31—C32 | 179.9 (2) |
O42—Mn3—O1—Mn2 | −39.09 (16) | Mn2—O31—C31—O32 | 19.9 (7) |
O61—Mn3—O1—Mn2 | −124.46 (16) | Mn2—O31—C31—C32 | −158.8 (3) |
O51—Mn3—O1—Mn2 | 138.25 (16) | O32—C31—C32—Cl31 | 16.1 (5) |
O32—Mn3—O1—Mn2 | 52.20 (16) | O31—C31—C32—Cl31 | −165.1 (3) |
O1—Mn1—O11—C11 | −0.6 (4) | O32—C31—C32—Cl33 | 138.1 (3) |
O62—Mn1—O11—C11 | −175.8 (6) | O31—C31—C32—Cl33 | −43.1 (4) |
O71—Mn1—O11—C11 | −179.6 (4) | O32—C31—C32—Cl32 | −103.2 (4) |
O21—Mn1—O11—C11 | −95.6 (4) | O31—C31—C32—Cl32 | 75.6 (4) |
O52—Mn1—O11—C11 | 93.2 (4) | Mn3—O42—C41—O41 | 36.2 (6) |
Mn2—Mn1—O11—C11 | −20.3 (3) | Mn3—O42—C41—C42 | −139.0 (3) |
O1—Mn2—O12—C11 | −27.3 (3) | Mn2—O41—C41—O42 | −9.2 (6) |
O22—Mn2—O12—C11 | 69.6 (3) | Mn2—O41—C41—C42 | 166.0 (3) |
O31—Mn2—O12—C11 | −123.1 (3) | O42—C41—C42—Cl42 | −156.2 (3) |
O81—Mn2—O12—C11 | 152.5 (3) | O41—C41—C42—Cl42 | 28.0 (5) |
Mn1—Mn2—O12—C11 | −4.7 (3) | O42—C41—C42—Cl41 | −32.6 (5) |
O1—Mn1—O21—C21 | −27.0 (3) | O41—C41—C42—Cl41 | 151.6 (3) |
O11—Mn1—O21—C21 | 68.8 (3) | O42—C41—C42—Cl43 | 85.4 (4) |
O62—Mn1—O21—C21 | −122.0 (3) | O41—C41—C42—Cl43 | −90.4 (4) |
O71—Mn1—O21—C21 | 154.2 (3) | Mn3—O51—C51—O52 | 30.6 (6) |
O52—Mn1—O21—C21 | 123.8 (6) | Mn3—O51—C51—C52 | −144.4 (3) |
Mn2—Mn1—O21—C21 | −5.5 (3) | Mn1—O52—C51—O51 | −6.4 (6) |
O1—Mn2—O22—C21 | 4.5 (4) | Mn1—O52—C51—C52 | 168.5 (2) |
O31—Mn2—O22—C21 | −177.4 (5) | O51—C51—C52—Cl53 | −39.4 (4) |
O81—Mn2—O22—C21 | −176.1 (4) | O52—C51—C52—Cl53 | 145.1 (3) |
O41—Mn2—O22—C21 | 97.4 (4) | O51—C51—C52—Cl52 | 79.0 (4) |
O12—Mn2—O22—C21 | −89.3 (4) | O52—C51—C52—Cl52 | −96.5 (4) |
Mn1—Mn2—O22—C21 | −14.4 (4) | O51—C51—C52—Cl51 | −160.8 (3) |
O1—Mn2—O31—C31 | 3.9 (4) | O52—C51—C52—Cl51 | 23.7 (5) |
O22—Mn2—O31—C31 | −174.2 (5) | Mn3—O61—C61—O62 | −7.0 (6) |
O81—Mn2—O31—C31 | −175.5 (4) | Mn3—O61—C61—C62 | 172.5 (3) |
O41—Mn2—O31—C31 | −90.1 (4) | Mn1—O62—C61—O61 | 30.8 (7) |
O12—Mn2—O31—C31 | 96.9 (4) | Mn1—O62—C61—C62 | −148.7 (3) |
Mn1—Mn2—O31—C31 | 24.2 (4) | O61—C61—C62—Cl61 | 5.9 (5) |
O42—Mn3—O32—C31 | 61.9 (3) | O62—C61—C62—Cl61 | −174.5 (3) |
O51—Mn3—O32—C31 | −124.0 (3) | O61—C61—C62—Cl63 | 127.2 (3) |
O91—Mn3—O32—C31 | 157.2 (3) | O62—C61—C62—Cl63 | −53.3 (4) |
O1—Mn3—O32—C31 | −31.6 (3) | O61—C61—C62—Cl62 | −114.3 (4) |
O1—Mn2—O41—C41 | −35.6 (3) | O62—C61—C62—Cl62 | 65.3 (4) |
O22—Mn2—O41—C41 | −132.0 (3) | Mn1—O71—C71—O72 | −9.1 (6) |
O31—Mn2—O41—C41 | 60.7 (3) | Mn1—O71—C71—C72 | 171.9 (3) |
O81—Mn2—O41—C41 | 144.6 (3) | Mn2—O81—C81—O82 | −14.4 (6) |
Mn1—Mn2—O41—C41 | −59.4 (3) | Mn2—O81—C81—C82 | 167.1 (3) |
O61—Mn3—O42—C41 | 80.0 (3) | Mn3—O91—C91—O92 | −34.0 (6) |
O91—Mn3—O42—C41 | 172.4 (3) | Mn3—O91—C91—C92 | 145.1 (4) |
O1—Mn3—O42—C41 | −11.4 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O72—H72···O52 | 0.78 (6) | 1.85 (6) | 2.621 (4) | 168 (6) |
O82—H82···O41 | 0.75 (6) | 1.98 (6) | 2.641 (4) | 149 (6) |
O92—H92···O32 | 0.72 (7) | 2.16 (7) | 2.815 (5) | 151 (7) |
C72—H72B···O91i | 0.98 | 2.37 | 3.142 (5) | 135 |
C72—H72C···O81ii | 0.98 | 2.46 | 3.367 (5) | 155 |
C92—H92C···O72iii | 0.98 | 2.52 | 3.243 (6) | 130 |
Symmetry codes: (i) x, y−1, z; (ii) x−1, y, z; (iii) x, y+1, z. |